HRID1757894

反应详情

EQUATION

反应方程式

HRID 1757894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 3.5 grams of 4,6-dichloro-2-isopropylamino-5-pyrimidinecarbonitrile in 100 ml of acetone was cooled to between 0° and -5°; a solution of 2.1 grams of aqueous 70% ethylamine in 25 ml of acetone was added dropwise. Upon complete addition, the reaction mixture was warmed to room temperature and stirred for 18 hours. The acetone was removed under reduced pressure, and the residue was extracted with a mixture of diethyl ether and water. The organic layer was separated and dried over magnesium sulfate. The mixture was filtered, and the filtrate was evaporated to dryness under reduced pressure. The residue was recrystallized from methylcyclohexane to give 3.1 grams of 4-chloro-6-ethylamino-2-isopropylamino-5-pyrimidinecarbonitrile; mp, 144°-146°.

WORKUP

后处理

  1. additionUpon complete addition
  2. customThe acetone was removed under reduced pressure
  3. extractionthe residue was extracted with a mixture of diethyl ether and water
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe mixture was filtered
  7. customthe filtrate was evaporated to dryness under reduced pressure
  8. customThe residue was recrystallized from methylcyclohexane